CN112979594B - Supercritical extraction process of andrographolide - Google Patents
Supercritical extraction process of andrographolide Download PDFInfo
- Publication number
- CN112979594B CN112979594B CN202110220915.3A CN202110220915A CN112979594B CN 112979594 B CN112979594 B CN 112979594B CN 202110220915 A CN202110220915 A CN 202110220915A CN 112979594 B CN112979594 B CN 112979594B
- Authority
- CN
- China
- Prior art keywords
- extraction
- macroporous resin
- elution
- resin purification
- liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/60—Two oxygen atoms, e.g. succinic anhydride
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses an andrographolide supercritical extraction process, which belongs to the technical field of extraction, wherein the extraction and purification rate of andrographolide is effectively enhanced to a certain extent by matching a supercritical CO2 extraction technology with an elution and purification technology of a macroporous resin purification layer, a plurality of macroporous resin purification layers are arranged in an elution device in an up-and-down stacking manner, an extraction mixed solution and a 45% ethanol solution are mixed and introduced into the elution device through a liquid inlet pipe, the mixed solution sequentially flows through the plurality of macroporous resin purification layers from top to bottom, the mixed extract is separated by ethanol elution on macroporous adsorption resin, ultrasonic vibrators are distributed among the plurality of macroporous resin purification layers in a staggered manner to synchronously carry out ultrasonic mixing and elution, thereby being more beneficial to fully separating extracted substances, and facilitating the increase of the yield of the prepared andrographolide, The purity is improved, and a product with high yield and high purity is obtained.
Description
Technical Field
The invention relates to the technical field of extraction, and particularly relates to an andrographolide supercritical extraction process.
Background
Andrographolide is an organic matter, natural plant andrographis paniculata whole plant can be used as a medicine, has the effects of clearing heat and removing toxicity, diminishing inflammation and cooling blood and stopping swelling, is widely applied to treatment of gastroenteritis, pneumonia, otitis media, bronchitis, dysentery, sphagitis, traumatic infection, water and fire scalds, snake venom bite, urinary tract infection, wind-heat type common cold, tonsillitis and the like, is known as a natural broad-spectrum antibiotic medicine, has the effects of clearing heat and removing toxicity, diminishing inflammation and relieving pain in clinical wide application, and has special curative effects on bacterial and viral upper respiratory tract infection and dysentery.
At present, the methods for extracting andrographolide are many, and the common methods include water extraction, alcohol extraction, supercritical extraction and the like. The water extraction method and the alcohol extraction method are most commonly used, but the two commonly used methods have certain defects: the extraction rate of andrographolide in the extract is low due to coarse process and more impurities, so that the purity is not high.
Therefore, we propose a supercritical extraction process of andrographolide to effectively solve some problems existing in the prior art.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide an andrographolide supercritical extraction process, which is characterized in that the extraction and purification rate of andrographolide is effectively enhanced to a certain extent by matching a supercritical CO2 extraction technology with an elution and purification technology of a macroporous resin purification layer, the macroporous resin purification layer is provided with a plurality of macroporous resin purification layers, the macroporous resin purification layers are arranged in an elution device in an up-and-down stacking manner, an extraction mixed solution and a 45% ethanol solution are mixed and guided into the elution device through a liquid inlet pipe, the mixed solution sequentially flows through the macroporous resin purification layers from top to bottom, the mixed extraction solution is eluted by ethanol on macroporous adsorption resin to achieve separation, ultrasonic vibrators are distributed among the macroporous resin purification layers in a staggered manner to synchronously carry out ultrasonic mixing and elution, thus being more beneficial to full separation among extraction substances and being convenient for increasing the yield of the prepared andrographolide, The purity is improved.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A supercritical extraction process of andrographolide comprises the following steps:
s1, placing the whole plant of andrographis paniculata into a crushing tank, adding cellulase, and crushing by a plant tissue crushing method to obtain an initial extraction solution;
s2, introducing the primary extraction liquid into an extractor, shunting and pressurizing the extractor, introducing CO2, heating the extractor by using a heating device to a supercritical temperature so as to realize that the primary extraction liquid and carbon dioxide reach the temperature required by supercritical extraction, and obtaining supercritical extraction liquid;
s3, introducing the supercritical extraction liquid obtained in the step S2 into a separator, adding 75% ethanol solution into the separator to dissolve, mix and dissolve, and extracting to obtain an extraction mixed liquid;
s4, preparing an elution device and a liquid collection cylinder, embedding and installing a plurality of macroporous resin purification layers in the elution device, wherein the macroporous resin purification layers are arranged in the elution device in an up-and-down stacked mode, introducing the extraction mixed liquid obtained in the step S3 into the elution device through a liquid inlet pipe, synchronously introducing 45% ethanol solution into the liquid inlet pipe through the ethanol liquid inlet pipe, and performing ultrasonic mixing elution by using a plurality of ultrasonic vibrators distributed among the macroporous resin purification layers in a staggered mode;
and S5, after the elution is finished, introducing the eluent into the liquid collecting barrel through a plurality of discharge valve ports on the elution device, recovering ethanol under reduced pressure, concentrating and drying to obtain the andrographolide extract.
Further, the extraction temperature in the S2 is 45-70 ℃, the extraction pressure is 25-45MPa, and the extraction time is 1-2.5 h.
Further, the CO2 in the S2 is cooled and liquefied by a cooling device before being introduced into the extractor, and the flow rate of the CO2 when being introduced into the extractor is 15-55L/h, so that the liquefied carbon dioxide meets the condition of being used as a solvent subsequently, and the pressurizing and conveying are facilitated to be smooth.
Furthermore, the eluter is a conical structure, the cross section area of the macroporous resin purification layer is sequentially reduced from top to bottom, the eluter is arranged in a conical structure, the mixed solution which is easy to extract is led out downwards, and the mixed solution flows through the macroporous resin purification layer in sequence for elution and adsorption.
Further, the bottom of feed liquor pipe is connected with communicating pipe through rotary joint, annular distribution has a plurality of liquid separating pipes, and is a plurality of on the lateral wall of communicating pipe the bottom of liquid separating pipe is equipped with the shower nozzle that is located top macroporous resin purification layer top, the bottom fixed connection of communicating pipe has rotatory bearing post, the bottom of rotatory bearing post runs through the bottom of elution ware and extends to in the liquid collecting barrel, the internally mounted of liquid collecting barrel has the linking post that carries out the bearing to rotatory bearing post, mixes the extract and leads to in the communicating pipe through the feed liquor pipe to spout on the macroporous resin purification layer through the shower nozzle of a plurality of liquid separating pipe bottoms, do benefit to the abundant diffusion of mixed extract.
Further, ethanol feed liquor union coupling is in top one side of feed liquor pipe, the top of feed liquor pipe is equipped with feed hopper, ethanol feed liquor pipe adopts hard pipe material to make, ethanol feed liquor pipe mounting is on external fixing device, and 45% ethanol solution leads to feed liquor pipe department through ethanol feed liquor pipe to derive through communicating pipe in the lump with the mixed extract of deriving downwards from feed hopper, be favorable to improving 45% ethanol solution and mixed extract and mix the degree of consistency, thereby improve the extraction effect.
Further, the top fixedly connected with ring rail of elution ware, be connected with the pole that links up through the sliding block on the ring rail, the outer end fixed connection that links up the pole utilizes the cooperation of ring rail and pole that links up for the rotation bearing post drives the communicating pipe on its top and rotates, further improves and can evenly spray from a plurality of shower nozzles spun solution and cover on macroporous resin purification layer.
Furthermore, the middle side wall of the plurality of macroporous resin purification layers is fixedly sleeved with a hollow sleeve, the hollow sleeve is connected with a rotary bearing column rotary sleeve, the outer side wall of the hollow sleeve is provided with an annular groove, the annular groove is internally and rotatably provided with a rotary sleeve, the ultrasonic vibrator is fixedly connected with the outer end of the rotary sleeve, the plurality of ultrasonic vibrators and the plurality of macroporous resin purification layers are arranged in a vertically staggered manner, the inner end of the rotary sleeve, which is connected with the ultrasonic vibrator, is embedded with a magnetic ball, the inner side of the rotary bearing column is provided with a hollow cavity, the inner wall of one end, which is close to the magnetic ball, of the hollow cavity is provided with a ferromagnetic driving ball, the ferromagnetic driving ball and the magnetic ball are arranged in a magnetic attraction manner, when the rotary bearing column rotates, the ferromagnetic driving ball inside the rotary bearing column can make a circular motion along with the magnetic ball when rotating along the axis of the rotary bearing column, thereby drive the ultrasonic vibrator in the swivel sleeve outside and make circular motion along rotatory bearing post to do benefit to and play the stirring effect to the extraction mixture material of leading-in to the elution ware, easily the extraction separation of material.
Further, ultrasonic vibrator includes the miniature supersonic generator of fixed connection and swivel sleeve outer end, miniature supersonic generator's outer end is equipped with the ultrasonic vibration pole, the ultrasonic vibration pole passes through cable electric connection with miniature supersonic generator, the annular distribution has a plurality of separation net strips on the lateral wall of ultrasonic vibration pole, and miniature supersonic generator realizes the ultrasonic vibration of ultrasonic vibration pole after the start-up to utilize the ultrasonic vibration effect, and cooperate its rotation operation, do benefit to the improvement to the purification rate of andrographolide.
Further, macroporous resin purification layer is round platform type structure, macroporous resin purification layer sets up from top to bottom including the fiber filtration layer that is located upper and lower layer be equipped with macroporous absorbent resin filling layer between the fiber filtration layer, and a plurality of macroporous resin purification layers are from last to the range upon range of setting up down, are favorable to enlarging macroporous absorbent resin's absorption purification area to effectively improve the purification rate.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) the scheme is matched with the elution purification technology of the macroporous resin purification layer by the supercritical CO2 extraction technology, the extraction and purification rate of the andrographolide is effectively enhanced to a certain degree, a plurality of macroporous resin purification layers are arranged, the macroporous resin purification layers are arranged in an elution device in an up-down stacking manner, the extraction mixed liquor and 45% ethanol solution are mixed and guided into the elution device through a liquid inlet pipe, the mixed solution sequentially flows through the macroporous resin purification layers from top to bottom, the mixed extract liquor is eluted by ethanol on macroporous adsorption resin to achieve separation, ultrasonic vibrators are distributed among the macroporous resin purification layers in a staggered manner, ultrasonic mixing elution is synchronously performed, sufficient separation of extracted substances is facilitated, so as to increase the yield and purity of the prepared andrographolide and obtain a high-yield and high-purity product.
(2) The extraction temperature in S2 is 45-70 ℃, the extraction pressure is 25-45MPa, the extraction time is 1-2.5h, CO2 in S2 is cooled and liquefied by a cooling device before being introduced into the extractor, and the flow rate of CO2 when being introduced into the extractor is 15-55L/h, so that the liquefied carbon dioxide meets the condition of using a subsequent solvent, and the smooth pressurizing and conveying are facilitated.
(3) The elutriator is the toper structure, a plurality of macroporous resin purification layers reduce from last to the sectional area down in proper order, set up the elutriator into the toper structure, easily extract the mixed liquid and derive downwards, and flow through macroporous resin purification layer in proper order and elute the absorption, macroporous resin purification layer is round platform type structure, macroporous resin purification layer is including the fiber filter layer that is located upper and lower floor, be equipped with the macroporous absorbent resin filling layer between the fiber filter layer that sets up from top to bottom, a plurality of macroporous resin purification layers are from last to range upon range of setting up down, be favorable to enlarging macroporous absorbent resin's absorption purification area, thereby effectively improve the purification rate.
(4) The bottom of feed liquor pipe is connected with communicating pipe through rotary joint, the annular distribution has a plurality of branch liquid pipes on the lateral wall of communicating pipe, a plurality of bottoms that divide the liquid pipe are equipped with the shower nozzle that is located top macroporous resin purification layer top, the bottom fixed connection of communicating pipe has rotatory bearing post, the bottom of rotatory bearing post is run through the bottom of elution ware and is extended to in the liquid collecting barrel, the internally mounted of liquid collecting barrel has the linking post that carries out the bearing to rotatory bearing post, it is intraductal to lead-in to the communicating pipe through the feed liquor pipe to mix the extract, and spout to macroporous resin purification layer on through the shower nozzle of a plurality of branch liquid pipe bottoms, do benefit to the abundant diffusion of mixing the extract.
(5) Ethanol feed liquor union coupling is in top one side of feed liquor pipe, the top of feed liquor pipe is equipped with feed hopper, ethanol feed liquor pipe adopts hard pipe material to make, ethanol feed liquor pipe is installed on external fixing device, 45% ethanol solution passes through the leading-in to feed liquor pipe department of ethanol feed liquor pipe, and derive through communicating pipe in the lump with the mixed extract of deriving downwards from feed hopper, be favorable to improving 45% ethanol solution and mixed extract mixing uniformity degree, thereby improve the extraction effect.
(6) The top fixedly connected with annular guide rail of elution ware is connected with the pole that links up through the sliding block on the annular guide rail, links up the outer end fixed connection of pole and on rotatory bearing post, utilizes annular guide rail and the cooperation of linking the pole for rotatory bearing post drives the communicating pipe on its top and rotates, further improves and can evenly spout from a plurality of shower nozzles spun solution and cover on macroporous resin purification layer.
(7) The middle side wall of each macroporous resin purification layer is fixedly sleeved with a hollow sleeve, the hollow sleeves are connected with a rotary bearing column rotary sleeve, the outer side wall of each hollow sleeve is provided with an annular groove, the rotary sleeves are rotatably installed in the annular groove, the ultrasonic vibrators are fixedly connected to the outer ends of the rotary sleeves and are arranged in a vertically staggered manner, the inner ends of the rotary sleeves, which are connected with the ultrasonic vibrators, are embedded with magnetic balls, the inner sides of the rotary bearing columns are provided with hollow cavities, the inner walls, close to one ends of the hollow cavities and the magnetic balls, are provided with ferromagnetic driving balls, the ferromagnetic driving balls and the magnetic balls are arranged in a magnetic attraction manner, when the rotary bearing column rotates, the ferromagnetic driving balls on the inner sides of the rotary bearing columns can make circular motion along the magnetic balls on the outer sides when rotating along the axial center of the rotary bearing column, thereby drive the ultrasonic vibrator in the swivel sleeve outside and make circular motion along rotatory bearing post to do benefit to and play the stirring effect to the extraction mixture material of leading-in to the elution ware, easily the extraction separation of material.
(8) Ultrasonic vibrator includes the miniature supersonic generator of fixed connection and swivel sleeve outer end, miniature supersonic generator's outer end is equipped with the ultrasonic vibration pole, the ultrasonic vibration pole passes through cable electric connection with miniature supersonic generator, the annular distribution has a plurality of separation net strips on the lateral wall of ultrasonic vibration pole, miniature supersonic generator is after the start-up, realize the ultrasonic vibration of ultrasonic vibration pole, utilize the ultrasonic vibration effect, and cooperate its rotation operation, do benefit to the improvement to the purification rate of andrographolide.
Drawings
FIG. 1 is a perspective view of the combination of the elutriator of the present invention and a macroporous resin purification layer;
FIG. 2 is a first perspective view of the junction of the macroporous resin purification layer and the ultrasonic vibrator of the present invention;
FIG. 3 is a second perspective view of the junction of the macroporous resin purification layer and the ultrasonic vibrator of the present invention;
FIG. 4 is a partial cross-sectional view at the macroporous resin purification layer of the present invention;
FIG. 5 is a perspective view of the rotary support post, hollow sleeve and ultrasonic vibrator configuration of the present invention;
fig. 6 is a partial internal cross-sectional view of the junction of the rotary support post, hollow sleeve and ultrasonic vibrator of the present invention.
The reference numbers in the figures illustrate:
the device comprises an eluter 1, a discharge valve port 101, a liquid collecting barrel 2, a rotary supporting column 3, a communicating pipe 4, a liquid inlet pipe 5, an annular guide rail 6, a connecting rod 601, an ethanol liquid inlet pipe 7, a liquid separating pipe 8, a spray head 9, a macroporous resin purification layer 10, a fiber filter layer 1001, a macroporous adsorption resin filling layer 1002, a hollow sleeve 11, a rotary sleeve 12, a miniature ultrasonic generator 13, an ultrasonic vibration rod 14, a separation mesh strip 15, a magnetic ball 16 and a ferromagnetic driving ball 17.
Detailed Description
The drawings in the embodiments of the invention will be combined; the technical scheme in the embodiment of the invention is clearly and completely described; obviously; the described embodiments are only some of the embodiments of the invention; but not all embodiments, are based on the embodiments of the invention; all other embodiments obtained by a person skilled in the art without making any inventive step; all fall within the scope of protection of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
referring to fig. 1, a supercritical extraction process of andrographolide includes the following steps:
s1, placing the whole plant of the common andrographis herb in a crushing tank, adding cellulase, crushing by a plant tissue crushing method to obtain primary extraction liquid, and breaking the cell wall of the whole plant of the common andrographis herb by combining the cellulase, thereby effectively increasing the diffusion and crushing area of effective components and improving the extraction rate of the effective components;
s2, introducing the primary extraction liquid into an extractor, shunting and pressurizing the extractor, introducing CO2, heating the extractor by using a heating device to a supercritical temperature so as to realize that the primary extraction liquid and carbon dioxide reach the temperature required by supercritical extraction, and obtaining supercritical extraction liquid;
s3, introducing the supercritical extraction liquid obtained in the step S2 into a separator, adding 75% ethanol solution into the separator to dissolve, mix and dissolve, and extracting to obtain an extraction mixed liquid;
s4, preparing an elution device 1 and a liquid collection cylinder 2, embedding a plurality of macroporous resin purification layers 10 in the elution device 1, stacking the macroporous resin purification layers 10 in the elution device 1 up and down, introducing the extraction mixed liquid obtained in the step S3 into the elution device 1 through a liquid inlet pipe 5, synchronously introducing 45% ethanol solution into the liquid inlet pipe 5 through an ethanol liquid inlet pipe 7, and performing ultrasonic mixing elution through a plurality of ultrasonic vibrators distributed among the macroporous resin purification layers 10 in a staggered mode;
and S5, after the elution is finished, introducing the eluent into the liquid collecting barrel 2 through a plurality of discharge valve ports 101 on the elution device 1, recovering ethanol under reduced pressure, concentrating and drying to obtain the andrographolide extract.
Wherein the extraction temperature in S2 is 45-70 ℃, the extraction pressure is 25-45MPa, the extraction time is 1-2.5h, CO2 in S2 is cooled and liquefied by a cooling device before being introduced into the extractor, and the flow rate of CO2 when being introduced into the extractor is 15-55L/h, so that the liquefied carbon dioxide meets the condition of using a subsequent solvent, and the smooth pressurizing and conveying are facilitated.
Referring to fig. 1-2, the elution apparatus 1 is a cone-shaped structure, the cross-sectional areas of a plurality of macroporous resin purification layers 10 are sequentially reduced from top to bottom, the elution apparatus 1 is arranged in a cone-shaped structure, the extraction mixture is easily led out downwards and flows through the macroporous resin purification layers 10 in sequence for elution and adsorption, the bottom end of the liquid inlet pipe 5 is connected with a communicating pipe 4 through a rotary joint, a plurality of liquid distributing pipes 8 are annularly distributed on the outer side wall of the communicating pipe 4, the bottom ends of the liquid distributing pipes 8 are provided with spray heads 9 positioned above the top macroporous resin purification layers 10, the bottom end of the communicating pipe 4 is fixedly connected with a rotary supporting column 3, the bottom end of the rotary supporting column 3 penetrates through the bottom of the elution apparatus 1 and extends into the liquid collecting cylinder 2, a connecting column for supporting the rotary supporting column 3 is arranged inside the liquid collecting cylinder 2, an ethanol liquid inlet pipe 7 is connected to one side of the top end of the liquid inlet pipe 5, and the top end of the liquid inlet pipe 5 is provided with a feeding funnel, ethanol feed liquor pipe 7 adopts hard pipe material to make, ethanol feed liquor pipe 7 is installed on external fixing device, rotary joint's setting, easily rotary support post 3 can not influence the installation of feed hopper and ethanol feed liquor pipe 7 isotructure when rotatory together with communicating pipe 4, 45% ethanol solution passes through ethanol feed liquor pipe 7 and leads to 5 departments of feed liquor pipe, and export through communicating pipe 4 with the mixed extract that derives downwards from feed hopper together, and spout on macroporous resin purification layer 10 through the shower nozzle 9 of 8 bottoms in a plurality of liquid distribution pipes, be favorable to improving 45% ethanol solution and mixed extract mixing degree of consistency, thereby improve the extraction effect, in the extraction separation process, close ejection of compact valve port 101, after this extraction stage finishes, open ejection of compact valve port 101 and carry out the material separation.
Referring to fig. 1 and 4, the top end of the elution device 1 is fixedly connected with an annular guide rail 6, the annular guide rail 6 is connected with an engaging rod 601 through a sliding block, the outer end of the engaging rod 601 is fixedly connected to the rotary supporting column 3, by the cooperation of the annular guide rail 6 and the engaging rod 601, the rotary supporting column 3 drives the communicating pipe 4 at the top end to rotate, so that the solution sprayed out of the plurality of spray heads 9 can be further improved to be uniformly sprayed on the macroporous resin purification layer 10, the macroporous resin purification layer 10 is of a round table structure, the macroporous resin purification layer 10 comprises fiber filter layers 1001 positioned on the upper layer and the lower layer, a macroporous adsorption resin filling layer 1002 is arranged between the fiber filter layers 1001 arranged on the upper layer and the lower layer, the plurality of macroporous resin purification layers 10 are stacked from top to bottom, and the adsorption purification area of the macroporous adsorption resin is favorably enlarged, thereby effectively improving the purification rate, and the mixed extract is eluted by certain ethanol on the macroporous absorption resin to achieve the purpose of separation.
Referring to fig. 1-3 and 5-6, the side wall of the middle part of the plurality of macroporous resin purification layers 10 is fixedly sleeved with a hollow sleeve 11, the hollow sleeve 11 is rotatably sleeved with a rotary supporting column 3 and connected, the outer side wall of the hollow sleeve 11 is provided with an annular groove, a rotary sleeve 12 is rotatably installed in the annular groove, an ultrasonic vibrator is fixedly connected to the outer end of the rotary sleeve 12, the plurality of ultrasonic vibrators and the plurality of macroporous resin purification layers 10 are arranged in a vertically staggered manner, the lengths of the plurality of ultrasonic vibrators are sequentially decreased from top to bottom so as to be matched with the macroporous resin purification layers 10 corresponding to the positions of the plurality of ultrasonic vibrators, a magnetic ball 16 is embedded at the inner end of the rotary sleeve 12 connected with the ultrasonic vibrator, a hollow cavity is arranged at the inner side of the rotary supporting column 3, a ferromagnetic driving ball 17 is installed on the inner wall of one end of the hollow cavity close to the magnetic ball 16, the ferromagnetic driving ball 17 is magnetically attracted to the magnetic ball 16, when rotatory bearing post 3 rotates, because ferromagnetic drive ball 17 and 16 magnetism of magnetic ball are inhaled the setting, the ferromagnetic drive ball 17 of 3 inboards of rotatory bearing post can make the magnetic ball 16 in the outside be circular motion along with it when rotatory along 3 axle centers of rotatory bearing post, thereby the ultrasonic vibrator who drives the 12 outsides of swivel sleeve is circular motion along rotatory bearing post 3, thereby do benefit to and play the stirring effect to leading-in extraction mixed material to the elution ware 1 in, the extraction separation of easy material, need here to supply be, 17 has the magnetism of certain strength to 16 and inhales the drive ability, easily drive ultrasonic vibrator and carry out rotary motion along with the axle center of rotatory bearing post 3.
Specifically, ultrasonic vibrator includes miniature supersonic generator 13 of fixed connection and 12 outer ends of swivel sleeve, the outer end of miniature supersonic generator 13 is equipped with ultrasonic vibration pole 14, miniature supersonic generator 13 has waterproof performance, ultrasonic vibration pole 14 passes through cable electric connection with miniature supersonic generator 13, annular distribution has a plurality of separation nettings 15 on the lateral wall of ultrasonic vibration pole 14, a plurality of meshs have been seted up on the separation nettings 15, miniature supersonic generator 13 is after the start-up, realize ultrasonic vibration of ultrasonic vibration pole 14, utilize the ultrasonic vibration effect, and cooperate its rotation operation, enlarge the ultrasonic range, do benefit to the abundant vibration of extraction mixed liquid molecule, aggravate the molecular motion, do benefit to the purification rate that improves andrographolide.
Compared with the extraction process of andrographolide in the prior art, the extraction and purification efficiency of andrographolide is effectively enhanced to a certain extent by matching the supercritical CO2 extraction technology with the elution and purification technology of the macroporous resin purification layer 10, the macroporous resin purification layers 10 are provided in plurality, the macroporous resin purification layers 10 are arranged in the elution device 1 in an up-down stacking manner, the extraction mixed solution is mixed with 45% ethanol solution and is introduced into the elution device 1, the mixed solution sequentially flows through the macroporous resin purification layers 10 from top to bottom, the mixed extract is separated on macroporous adsorption resin by eluting with ethanol in a certain amount, and ultrasonic mixing elution is synchronously performed, so that the separation of extracted substances is facilitated, the increase of the yield of the prepared andrographolide and the improvement of the purity are facilitated;
after the use is finished, the rotary supporting columns 3, the communicating pipes 4 and other structures are upwards disassembled, so that the plurality of macroporous resin purification layers 10 in the elution device 1 can be conveniently disassembled, and the subsequent cleaning and the replacement of the macroporous resin purification layers 10 are convenient.
The above; but are merely preferred embodiments of the invention; the scope of the invention is not limited thereto; any person skilled in the art is within the technical scope of the present disclosure; the technical scheme and the improved concept of the invention are equally replaced or changed; are intended to be covered by the scope of the present invention.
Claims (6)
1. A supercritical extraction process of andrographolide is characterized in that: the method comprises the following steps:
s1, placing the whole plant of andrographis paniculata into a crushing tank, adding cellulase, and crushing by a plant tissue crushing method to obtain an initial extraction solution;
s2, introducing the primary extraction liquid into an extractor, shunting and pressurizing the extractor, introducing CO2, heating the extractor by using a heating device to a supercritical temperature so as to realize that the primary extraction liquid and carbon dioxide reach the temperature required by supercritical extraction, and obtaining supercritical extraction liquid;
s3, introducing the supercritical extraction liquid obtained in the step S2 into a separator, adding 75% ethanol solution into the separator, mixing and dissolving, and extracting to obtain an extraction mixed liquid;
s4, preparing an elution device (1) and a liquid collection cylinder (2), embedding and installing a plurality of macroporous resin purification layers (10) in the elution device (1), stacking the macroporous resin purification layers (10) in the elution device (1) up and down, introducing the extraction mixed liquid obtained in the step S3 into the elution device (1) through a liquid inlet pipe (5), synchronously introducing 45% ethanol solution into the liquid inlet pipe (5) through an ethanol liquid inlet pipe (7), and performing ultrasonic mixing elution by utilizing a plurality of ultrasonic vibrators distributed among the macroporous resin purification layers (10) in a staggered manner;
s5, after the elution is finished, introducing the eluent into the liquid collecting barrel (2) through a plurality of discharge valve ports (101) on the elution device (1), recovering ethanol under reduced pressure, concentrating and drying to obtain an andrographolide extract;
the bottom of feed liquor pipe (5) is connected with communicating pipe (4) through rotary joint, the annular distributes on the lateral wall of communicating pipe (4) has a plurality of branch liquid pipes (8), a plurality of the bottom of dividing liquid pipe (8) is equipped with shower nozzle (9) that are located top macroporous resin purification layer (10) top, the bottom fixed connection of communicating pipe (4) has rotatory bearing post (3), the bottom of rotatory bearing post (3) runs through the bottom of elution ware (1) and extends to in liquid collecting barrel (2), the internally mounted of liquid collecting barrel (2) has the linking post that carries on supporting to rotatory bearing post (3), ethanol feed liquor pipe (7) is connected in feed liquor pipe (5) top one side, the top of feed liquor pipe (5) is equipped with feed hopper, ethanol feed liquor pipe (7) adopt the hard pipe material to make, ethanol feed liquor pipe (7) are installed on external fixing device, the top fixedly connected with ring rail (6) of elution ware (1), be connected with joint pole (601) through the sliding block on ring rail (6), the outer end fixed connection who links up pole (601) is on rotatory bearing post (3), and is a plurality of all fixed cover is equipped with well hollow sleeve (11) on the middle part lateral wall of macroporous resin purification layer (10), well hollow sleeve (11) establish the link with rotatory bearing post (3) rotating sleeve, seted up the ring channel on the lateral wall of well hollow sleeve (11), swivel sleeve (12) is installed to the ring channel internal rotation, ultrasonic vibrator fixed connection is in the outer end of swivel sleeve (12), and crisscross setting about a plurality of ultrasonic vibrator and a plurality of macroporous resin purification layer (10), the inner that swivel sleeve (12) and ultrasonic vibrator linked up mutually inlays to establish and installs magnetic ball (16), well cavity has been seted up to the inboard of rotatory bearing post (3), the inner wall of one end of the hollow cavity close to the magnetic ball (16) is provided with a ferromagnetic driving ball (17), and the ferromagnetic driving ball (17) and the magnetic ball (16) are arranged in a magnetic attraction mode.
2. The supercritical extraction process of andrographolide according to claim 1, wherein: the extraction temperature in the S2 is 45-70 ℃, the extraction pressure is 25-45MPa, and the extraction time is 1-2.5 h.
3. The supercritical extraction process of andrographolide according to claim 1, wherein: and the CO2 in the S2 is cooled and liquefied by a cooling device before being introduced into the extractor, and the flow rate of the CO2 when being introduced into the extractor is 15-55L/h.
4. The supercritical extraction process of andrographolide according to claim 1, wherein: the elution device (1) is of a conical structure, and the cross sections of the macroporous resin purification layers (10) are sequentially reduced from top to bottom.
5. The supercritical extraction process of andrographolide according to claim 1, wherein: ultrasonic vibrator includes miniature supersonic generator (13) of fixed connection and swivel sleeve (12) outer end, the outer end of miniature supersonic generator (13) is equipped with ultrasonic vibration pole (14), ultrasonic vibration pole (14) pass through cable electric connection with miniature supersonic generator (13), annular distribution has a plurality of separation nettings (15) on the lateral wall of ultrasonic vibration pole (14).
6. The supercritical extraction process of andrographolide according to claim 1, wherein: the macroporous resin purification layer (10) is of a round table structure, the macroporous resin purification layer (10) comprises fiber filtering layers (1001) which are arranged at the upper layer and the lower layer, and a macroporous adsorption resin filling layer (1002) is arranged between the fiber filtering layers (1001) which are arranged up and down.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110220915.3A CN112979594B (en) | 2021-02-26 | 2021-02-26 | Supercritical extraction process of andrographolide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110220915.3A CN112979594B (en) | 2021-02-26 | 2021-02-26 | Supercritical extraction process of andrographolide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112979594A CN112979594A (en) | 2021-06-18 |
| CN112979594B true CN112979594B (en) | 2021-12-14 |
Family
ID=76351281
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110220915.3A Active CN112979594B (en) | 2021-02-26 | 2021-02-26 | Supercritical extraction process of andrographolide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112979594B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114507198A (en) * | 2022-04-02 | 2022-05-17 | 江西成必信生物科技有限公司 | Andrographolide extraction process |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435578A (en) * | 2013-09-17 | 2013-12-11 | 南京通泽农业科技有限公司 | Method for extracting andrographolide from andrographis paniculata |
| CN103483299A (en) * | 2013-10-08 | 2014-01-01 | 南京正亮医药科技有限公司 | Extraction method and application of andrographolide |
| CN103664842A (en) * | 2013-12-16 | 2014-03-26 | 无锡济民可信山禾药业股份有限公司 | Continuous chromatographic separation method for andrographolide |
| CN104307205A (en) * | 2014-11-12 | 2015-01-28 | 成都彼斯特生物科技有限公司 | Macroporous resin adsorption-separation device |
| CN105477902A (en) * | 2015-12-23 | 2016-04-13 | 江苏七O七天然制药有限公司 | Extracting separating device by utilization of impregnation method |
| CN105968146A (en) * | 2016-05-11 | 2016-09-28 | 张铰铣 | Tea polyphenol production process for producing plurality of products by one time of feeding |
| CN106807114A (en) * | 2015-11-30 | 2017-06-09 | 中美华世通生物医药科技（武汉）有限公司 | Taper chromatographic fractionation system and its method for isolating and purifying |
| CN107746395A (en) * | 2017-10-23 | 2018-03-02 | 吉林大学珠海学院 | A kind of method of andrographolide in extraction chuanxinlian tablet |
| CN109158096A (en) * | 2018-10-29 | 2019-01-08 | 江苏九九久科技有限公司 | Accelerate the method for macroporous resin adsorption and desorption rate |
| CN208959367U (en) * | 2018-03-03 | 2019-06-11 | 四川子仁制药有限公司 | A kind of andrographolide refining system |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100666652B1 (en) * | 2000-02-25 | 2007-01-09 | 한화석유화학 주식회사 | Method for preparing taxol using supercritical fluid from plant |
-
2021
- 2021-02-26 CN CN202110220915.3A patent/CN112979594B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435578A (en) * | 2013-09-17 | 2013-12-11 | 南京通泽农业科技有限公司 | Method for extracting andrographolide from andrographis paniculata |
| CN103483299A (en) * | 2013-10-08 | 2014-01-01 | 南京正亮医药科技有限公司 | Extraction method and application of andrographolide |
| CN103664842A (en) * | 2013-12-16 | 2014-03-26 | 无锡济民可信山禾药业股份有限公司 | Continuous chromatographic separation method for andrographolide |
| CN104307205A (en) * | 2014-11-12 | 2015-01-28 | 成都彼斯特生物科技有限公司 | Macroporous resin adsorption-separation device |
| CN106807114A (en) * | 2015-11-30 | 2017-06-09 | 中美华世通生物医药科技（武汉）有限公司 | Taper chromatographic fractionation system and its method for isolating and purifying |
| CN105477902A (en) * | 2015-12-23 | 2016-04-13 | 江苏七O七天然制药有限公司 | Extracting separating device by utilization of impregnation method |
| CN105968146A (en) * | 2016-05-11 | 2016-09-28 | 张铰铣 | Tea polyphenol production process for producing plurality of products by one time of feeding |
| CN107746395A (en) * | 2017-10-23 | 2018-03-02 | 吉林大学珠海学院 | A kind of method of andrographolide in extraction chuanxinlian tablet |
| CN208959367U (en) * | 2018-03-03 | 2019-06-11 | 四川子仁制药有限公司 | A kind of andrographolide refining system |
| CN109158096A (en) * | 2018-10-29 | 2019-01-08 | 江苏九九久科技有限公司 | Accelerate the method for macroporous resin adsorption and desorption rate |
Non-Patent Citations (1)
| Title |
|---|
| Technical optimization of the extraction of andrographolide by supercritical CO2;Kexun Chen 等;《Food and Bioproducts Processing》;20111231;第89卷;第92-97页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112979594A (en) | 2021-06-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108314608B (en) | Extraction and separation method of cannabidiol | |
| CN109053388A (en) | A method of extracting cannabidiol | |
| CN112979594B (en) | Supercritical extraction process of andrographolide | |
| CN110075567A (en) | A kind of high-pressure fog combines the centrifugal device and method of adverse current precipitating | |
| CN101812100A (en) | Method for preparing icariin | |
| CN108017530A (en) | A kind of method that Co-Q10 is continuously separated from bacteria residue | |
| CN107698691A (en) | A kind of separating and purifying flavone from oldenlandia diffusa, the system and method for polysaccharide | |
| CN110507636A (en) | Andrographolide dry suspensoid agent preparation method | |
| CN108771623A (en) | A kind of Chinese medicine crushing extraction element | |
| CN207614488U (en) | Ultrafiltration membrane separating device for saponin(e purification | |
| CN106916162B (en) | A kind of preparation method of jolkinolide B bulk pharmaceutical chemicals | |
| CN109810087B (en) | Compound for preventing and treating alcoholism and preparation method thereof | |
| CN210751382U (en) | Effective component extraction element is used in chinese herbal medicine processing | |
| CN107286266A (en) | Extract the extraction equipment and its extracting method of red bayberry polysaccharide | |
| CN103030674B (en) | In a kind of wintergreen, extract the production method of Hyperoside | |
| CN111840353A (en) | Preparation method and equipment of elderberry extract | |
| CN207512110U (en) | The device of high-purity tacrolimus is extracted from fermentation mycelium | |
| CN205287148U (en) | Hydrogen therapeutic apparatus | |
| CN218358506U (en) | Medicine separation, concentration and purification equipment | |
| CN218841783U (en) | Redistribution device for desulfurization waste liquid absorption tower | |
| CN108635960A (en) | A kind of Tea Samples rapid filtering device | |
| CN220715015U (en) | Traditional chinese medicine liquid filter equipment | |
| CN208482048U (en) | A kind of extraction element of suitable thermal sensitivity chemical composition of Chinese materia medica | |
| CN219804269U (en) | Filter equipment is used in production of spring jade liquid | |
| CN214508593U (en) | Irrigation equipment is used in farmland construction |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |